Acetic Acid → HCID 54152829, compound

Participants

Reaction Conditions

Reaction Steps

21.8 ml of n-butyllithium solution (2.2M in hexane) are added dropwise at -65° C. to a solution of 5.58 g of methanephosphonic acid dimethyl ester in 160 ml of absolute tetrahydrofuran and the mixture is stirred at that temperature for 15 minutes. A solution of 4.05 g of the methyl ester obtained in Example (6d) in 10 ml of tetrahydrofuran is then added and the mixture is stirred at -65° C. for 1 hour. The solution is heated to -10° C., 2.80 ml of acetic acid are added and the mixture is concentrated. The residue is partitioned between ethene and water, the ether phase is separated, dried over magnesium sulphate and concentrated in vacuo. The residue is then purified by ball-tube distillation. 4.23 g of the title compound are obtained (bath temperature 180°-185° C., 1.5 torr).

Provenance & Evidence